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CN109234560A - A kind of Ta-W-Al-Al2O3Alloy bar material and preparation method - Google Patents

A kind of Ta-W-Al-Al2O3Alloy bar material and preparation method Download PDF

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Publication number
CN109234560A
CN109234560A CN201811168573.XA CN201811168573A CN109234560A CN 109234560 A CN109234560 A CN 109234560A CN 201811168573 A CN201811168573 A CN 201811168573A CN 109234560 A CN109234560 A CN 109234560A
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China
Prior art keywords
powder
bar material
alloy bar
shell
alloy
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CN201811168573.XA
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Inventor
常喜
周刚
王占锋
张力力
卢成成
梁宏裕
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Xi'an Huashan Metal Product Co Ltd
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Xi'an Huashan Metal Product Co Ltd
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Priority to CN201811168573.XA priority Critical patent/CN109234560A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/20Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02Alloys based on vanadium, niobium, or tantalum

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a kind of Ta-W-Al-Al2O3Alloy bar material and preparation method, it is related to alloy bar material technical field.It is made of the raw material of following mass percent: W 5%-15%, Al 2%-6%, Al2O31%-4%, surplus Ta, preparation method are as follows: tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, ball milling mixing is uniform under argon atmosphere protection, obtains mixed-powder;Compression moulding obtains blank;Blank is fitted into shell, sealed after being vacuumized shell;HIP sintering obtains Ta-W-Al-Al2O3Alloy sintered compact;Hot extrusion obtains Ta-W-Al-Al2O3Alloy bar material.Alloy bar material prepared by the present invention has good temperature-room type plasticity and tensile strength and excellent high temperature intensity and antioxygenic property, can use in 1500 DEG C of air environments.

Description

A kind of Ta-W-Al-Al2O3Alloy bar material and preparation method
Technical field
The present invention relates to alloy bar material technical fields, and in particular to a kind of Ta-W-Al-Al2O3Alloy bar material and preparation Method.
Background technique
Tantalum alloy has many advantages, such as the high and good processing performance of high density, high temperature resistant, intensity, fracture toughness, corrosion resistance, It is the indispensable important materials in the fields such as Aeronautics and Astronautics, chemical industry, nuclear industry, high-temperature technology, has a good application prospect. Tantalum-tungsten alloy is used for the superhigh temperature structural member of the extreme environments such as superhigh temperature, super-pressure, high-speed flow erosion, rapid heat cycle more On, it is such as used for rocket engine high-temperature structural material, the heat of the heat-resisting covering of hypersonic reentry vehicles, space shuttle to be anti- Shield, cladding nuclear fuels material, the control zero of the rudder piece, supersonic plane combustion chamber, rocket, guided missile and jet engine of anti-ablation Part and regulating device part.
However, the elevated temperature strength of tantalum-tungsten alloy is remarkably decreased, and alloy is added in tantalum when being more than 1200 DEG C using temperature Element can form the high tantalum alloy of alloy concentrations, and mechanical behavior under high temperature significantly improves, and processing performance is good, therefore be used as height Warm structural material, although tantalum alloy mechanical behavior under high temperature can be made to obtain a degree of improvement by alloying, substantially Improve the limited promise that its mechanical property makes it be applied under superhigh temperature adverse circumstances.Meanwhile the preparation side of tantalum-tungsten alloy Electro-bombardment melting method is usually used in method, and tantalum alloy ingot casting coarse grains, averagely reach 3- made from electro-bombardment melting method 5mm, this is unfavorable to the mechanical property of material.In addition, easily oxygen uptake occurs when tantalum-tungsten alloy is exposed in 300 DEG C or more of air Oxidation, which also limits the applications of tantalum-tungsten alloy.Therefore, it is necessary to overcome single-phase tantalum-tungsten alloy by second-phase dispersion reinforcing Disadvantage, design increase ceramic phase in tantalum-tungsten alloy, and by alloying and technology controlling and process, make ceramic phase fine particle uniformly more It is dispersed on tantalum matrix, so that its room-temperature mechanical property, mechanical behavior under high temperature and high-temperature oxidation resistance be made to be significantly improved.Base In this, designs a kind of Ta-W-Al-Al2O3 alloy bar material and preparation method is particularly necessary.
Summary of the invention
In view of the shortcomings of the prior art, object of the present invention is to be to provide a kind of Ta-W-Al-Al2O3Alloy bar Material and preparation method, the Ta-W-Al-Al of this method preparation2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Different Testing Tensile Strength at Elevated Temperature and antioxygenic property can use in 1500 DEG C of air environments.
To achieve the goals above, the present invention is to realize by the following technical solutions: a kind of Ta-W-Al-Al2O3It closes Golden bar is made of the raw material of following mass percent: W 5%-15%, Al 2%-6%, Al2O31%-4%, surplus Ta; Described W, Al, the Al2O3, Ta be powder raw material, wherein the granularity of W powder and Al powder is no more than 30 μm, Al2O3The grain of powder Degree is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;W powder, Al powder and the Al2O3The quality purity of powder is not less than The quality purity of 99.9%, Ta powder is not less than 99.5%.
Preferably, the Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 8%- 12%, Al 3%-5%, Al2O32%-3%, surplus Ta.
Preferably, the Ta-W-Al-Al2O3Alloy bar material is made: W of the raw material of following mass percent 10%, Al 4%, Al2O32.5%, surplus Ta.
A kind of Ta-W-Al-Al2O3The preparation method of alloy bar material, preparation step are as follows:
(1) by W, Al, Al2O3It is placed in ball mill with Ta, ball milling mixing is uniform under argon atmosphere protection, is mixed Powder;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into shell, shell is vacuumized, seal casinghousing after the intracorporal air of shell to be evacuated;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1500 DEG C -1700 DEG C, pressure is HIP sintering 1h-3h under conditions of 160MPa-200MPa removes shell after natural cooling, obtains Ta-W-Al-Al2O3It closes Golden sintered body;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1400 DEG C -1600 DEG C, extrusion ratio 6-10 Under conditions of squeezed, the processing that strips off the skin is carried out after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Preferably, the rotational speed of ball-mill of ball mill is 200r/min-400r/min, the time of ball milling in the step (1) For 6h-12h.
Preferably, shell is hollow cylindrical structure in the step (3), the material of shell is pure titanium.
Preferably, Ta-W-Al-Al in the step (5)2O3The extruding temperature preferred scope of alloy sintered compact is 1450 DEG C -1550 DEG C, extrusion ratio 7-9.
Beneficial effects of the present invention: the Ta-W-Al-Al of this method preparation2O3Alloy bar material room temperature tensile intensity is 578MPa-865MPa, room temperature elongation percentage are 16%-27%, and 1700 DEG C of tensile strength is 355MPa-439MPa, at 1500 DEG C Material loss is 0.60mg/cm after aoxidizing 100h in air environment2-0.31mg/cm2, the Ta-W-Al-Al2O3Alloy bar material tool There are good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and antioxygenic property, it can be in 1500 DEG C of air rings It is used in border.
Detailed description of the invention
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments;
Fig. 1 is Ta-W-Al-Al prepared by the embodiment of the present invention 12O3The micro-organization chart of alloy bar material.
Specific embodiment
To be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, below with reference to Specific embodiment, the present invention is further explained.
Referring to Fig.1, present embodiment uses a kind of following technical scheme: Ta-W-Al-Al2O3Alloy bar material, by with The raw material of lower mass percent is made: W 5%-15%, Al 2%-6%, Al2O31%-4%, surplus Ta;The W, Al、Al2O3, Ta be powder raw material, wherein the granularity of W powder and Al powder is no more than 30 μm, Al2O3The granularity of powder is not more than 10 μm, the granularity of Ta powder is not more than 50 μm;W powder, Al powder and the Al2O3The quality purity of powder is not less than 99.9%, The quality purity of Ta powder is not less than 99.5%.
A kind of Ta-W-Al-Al2O3The preparation method of alloy bar material, preparation step are as follows:
(1) by W, Al, Al2O3It is placed in ball mill with Ta, ball milling mixing is uniform under argon atmosphere protection, is mixed Powder;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into shell, shell is vacuumized, seal casinghousing after the intracorporal air of shell to be evacuated;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1500 DEG C -1700 DEG C, pressure is HIP sintering 1h-3h under conditions of 160MPa-200MPa removes shell after natural cooling, obtains Ta-W-Al-Al2O3It closes Golden sintered body;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1400 DEG C -1600 DEG C, extrusion ratio 6-10 Under conditions of squeezed, the processing that strips off the skin is carried out after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
It is worth noting that, the rotational speed of ball-mill of ball mill is 200r/min-400r/min, ball milling in the step (1) Time be 6h-12h.
Shell is hollow cylindrical structure in the step (3), and the material of shell is pure titanium.
Ta-W-Al-Al in the step (5)2O3The extruding temperature preferred scope of alloy sintered compact is 1450 DEG C -1550 DEG C, extrusion ratio 7-9.
Al element is added to Ta-W-Al-Al by present embodiment2O3In alloy, due to Al element have with oxygen it is very high Affinity, therefore Al element will reduce the oxygen content of Ta matrix, reduce oxygen element to the adverse effect of alloy, and improve Ta-W-Al-Al2O3The high-temperature oxidation resistance of alloy, while the present invention is directed to the deficiency of existing tantalum alloy bar, is dissolved using W Strengthen, Al2O3Second-phase dispersion is strengthened, and prepares Ta-W-Al-Al by hot isostatic pressing+hot extrusion technique process2O3Alloy bar Material makes small Al2O3Ceramic phase particles even dispersion is distributed on Ta matrix, to make Ta-W-Al-Al2O3Alloy bar material Room-temperature mechanical property, mechanical behavior under high temperature and antioxygenic property are significantly improved.
Present embodiment prepares Ta-W-Al-Al using hot isostatic pressing+hot extrusion technique process2O3Alloy bar material, Room temperature tensile intensity is 578MPa-865MPa, room temperature elongation percentage is 16%-27%, and 1700 DEG C of tensile strength is 355MPa- 439MPa, material loss is 0.60mg/cm after 100h is aoxidized in 1500 DEG C of air environments2-0.31mg/cm2, the Ta-W-Al- Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and antioxygenic property, can It is used in 1500 DEG C of air environments.
A kind of embodiment 1: Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 10%, Al 4%, Al2O32.5%, surplus Ta, wherein described W, Al, Al2O3, Ta be powder raw material, the granularity of W powder and Al powder is equal No more than 30 μm, Al2O3The granularity of powder is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;The W powder, Al powder and Al2O3The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
The Ta-W-Al-Al2O3The preparation step of alloy bar material are as follows:
(1) tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, the ball milling under argon atmosphere protection It is uniformly mixed, obtains mixed-powder, wherein the rotational speed of ball-mill of ball mill is 300r/min, and the time of the ball milling is 8h;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into the pure titanium shell of hollow cylindrical structure, shell is vacuumized, shell to be evacuated is intracorporal Seal casinghousing after air;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1600 DEG C, pressure is 180MPa's Under the conditions of HIP sintering 1.5h, remove shell after natural cooling, obtain Ta-W-Al-Al2O3Alloy sintered compact;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1500 DEG C, extrusion ratio is 8 under conditions of into Row squeezes, and carries out the processing that strips off the skin after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3The microscopic structure of alloy bar material is as shown in Figure 1, it can be seen that this Ta- W-Al-Al2O3Alloy bar material microstructure be not observed cavity, micro-crack the defects of, material is almost fine and close, this be by In Ta-W-Al-Al2O3Alloy bar material uses hot isostatic pressing+hot extrusion technique process during the preparation process, not only eliminates material Defect produced during the preparation process, and crystal grain is reset in hot extrusion process, makes tiny Al2O3Ceramic particle is uniform It is distributed in Ta matrix, tiny Al2O3Ceramic phase particles generate strong reinforcing to Ta matrix grain and crystal boundary, therefore, greatly Improve Ta-W-Al-Al2O3The room-temperature mechanical property and elevated temperature strength of alloy bar material.Further, since W element solid solution is in Ta, Solution strengthening is generated to Ta, also significantly increases the room temperature and mechanical behavior under high temperature of material;Al element solid solution is in Ta, in high temperature One layer of fine and close oxidation film is formed in oxidizing atmosphere, is prevented the intrusion of oxygen, is protected the surface of material, improve Ta-W-Al- Al2O3The antioxygenic property of alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3Alloy bar material, room temperature tensile intensity are 865MPa, room temperature elongation percentage It is 27%, 1700 DEG C of tensile strength is 439MPa, and material loss is 0.31mg/ after 100h is aoxidized in 1500 DEG C of air environments cm2, the Ta-W-Al-Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and anti- Oxidation susceptibility can use in 1500 DEG C of air environments.
A kind of embodiment 2: Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 5%, Al 2%, Al2O31%, surplus Ta, wherein described W, Al, Al2O3, Ta be powder raw material, the granularity of W powder and Al powder is not Greater than 30 μm, Al2O3The granularity of powder is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;W powder, Al powder and the Al2O3 The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
The Ta-W-Al-Al2O3The preparation step of alloy bar material are as follows:
(1) tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, the ball milling under argon atmosphere protection It is uniformly mixed, obtains mixed-powder, wherein the rotational speed of ball-mill of ball mill is 200r/min, and the time of the ball milling is 6h;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into the pure titanium shell of hollow cylindrical structure, shell is vacuumized, shell to be evacuated is intracorporal Seal casinghousing after air;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1500 DEG C, pressure is 160MPa's Under the conditions of HIP sintering 1h, remove shell after natural cooling, obtain Ta-W-Al-Al2O3Alloy sintered compact;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1400 DEG C, extrusion ratio is 6 under conditions of into Row squeezes, and carries out the processing that strips off the skin after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3Alloy bar material, room temperature tensile intensity are 578MPa, room temperature elongation percentage It is 16%, 1700 DEG C of tensile strength is 355MPa, and material loss is 0.60mg/ after 100h is aoxidized in 1500 DEG C of air environments cm2, the Ta-W-Al-Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and anti- Oxidation susceptibility can use in 1500 DEG C of air environments.
A kind of embodiment 3: Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 15%, Al 6%, Al2O34%, surplus Ta, wherein described W, Al, Al2O3, Ta be powder raw material, the granularity of W powder and Al powder is not Greater than 30 μm, Al2O3The granularity of powder is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;W powder, Al powder and the Al2O3 The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
The Ta-W-Al-Al2O3The preparation step of alloy bar material are as follows:
(1) tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, the ball milling under argon atmosphere protection It is uniformly mixed, obtains mixed-powder, wherein the rotational speed of ball-mill of ball mill is 400r/min, and the time of the ball milling is 12h;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into the pure titanium shell of hollow cylindrical structure, shell is vacuumized, shell to be evacuated is intracorporal Seal casinghousing after air;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1700 DEG C, pressure is 200MPa's Under the conditions of HIP sintering 3h, remove shell after natural cooling, obtain Ta-W-Al-Al2O3Alloy sintered compact;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact is under conditions of extruding temperature is 1600 DEG C, extrusion ratio is 10 It is squeezed, the processing that strips off the skin is carried out after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3Alloy bar material, room temperature tensile intensity are 712MPa, room temperature elongation percentage It is 23%, 1700 DEG C of tensile strength is 389MPa, and material loss is 0.55mg/ after 100h is aoxidized in 1500 DEG C of air environments cm2, the Ta-W-Al-Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and anti- Oxidation susceptibility can use in 1500 DEG C of air environments.
A kind of embodiment 4: Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 8%, Al 3%, Al2O32%, surplus Ta, wherein described W, Al, Al2O3, Ta be powder raw material, the granularity of W powder and Al powder is not Greater than 30 μm, Al2O3The granularity of powder is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;W powder, Al powder and the Al2O3 The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
The Ta-W-Al-Al2O3The preparation step of alloy bar material are as follows:
(1) tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, the ball milling under argon atmosphere protection It is uniformly mixed, obtains mixed-powder, wherein the rotational speed of ball-mill of ball mill is 400r/min, and the time of the ball milling is 12h;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into the pure titanium shell of hollow cylindrical structure, shell is vacuumized, shell to be evacuated is intracorporal Seal casinghousing after air;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1700 DEG C, pressure is 200MPa's Under the conditions of HIP sintering 3h, remove shell after natural cooling, obtain Ta-W-Al-Al2O3Alloy sintered compact;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact is under conditions of extruding temperature is 1600 DEG C, extrusion ratio is 10 It is squeezed, the processing that strips off the skin is carried out after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3Alloy bar material, room temperature tensile intensity are 720MPa, room temperature elongation percentage It is 23%, 1700 DEG C of tensile strength is 389MPa, and material loss is 0.57mg/ after 100h is aoxidized in 1500 DEG C of air environments cm2, the Ta-W-Al-Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and anti- Oxidation susceptibility can use in 1500 DEG C of air environments.
A kind of embodiment 5: Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 12%, Al 5%, Al2O33%, surplus Ta, wherein described W, Al, Al2O3, Ta be powder raw material, the granularity of W powder and Al powder is not Greater than 30 μm, Al2O3The granularity of powder is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;W powder, Al powder and the Al2O3 The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
The Ta-W-Al-Al2O3The preparation step of alloy bar material are as follows:
(1) tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, the ball milling under argon atmosphere protection It is uniformly mixed, obtains mixed-powder, wherein the rotational speed of ball-mill of ball mill is 300r/min, and the time of the ball milling is 8h;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into the pure titanium shell of hollow cylindrical structure, shell is vacuumized, shell to be evacuated is intracorporal Seal casinghousing after air;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1600 DEG C, pressure is 180MPa's Under the conditions of HIP sintering 1.5h, remove shell after natural cooling, obtain Ta-W-Al-Al2O3Alloy sintered compact;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1500 DEG C, extrusion ratio is 8 under conditions of into Row squeezes, and carries out the processing that strips off the skin after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3Alloy bar material, room temperature tensile intensity are 635MPa, room temperature elongation percentage It is 25%, 1700 DEG C of tensile strength is 410MPa, and material loss is 0.55mg/ after 100h is aoxidized in 1500 DEG C of air environments cm2, the Ta-W-Al-Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and anti- Oxidation susceptibility can use in 1500 DEG C of air environments.
A kind of embodiment 6: Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 10%, Al 4%, Al2O32.5%, surplus Ta, wherein described W, Al, Al2O3, Ta be powder raw material, the granularity of W powder and Al powder is equal No more than 30 μm, Al2O3The granularity of powder is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;The W powder, Al powder and Al2O3The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
The Ta-W-Al-Al2O3The preparation step of alloy bar material are as follows:
(1) tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, the ball milling under argon atmosphere protection It is uniformly mixed, obtains mixed-powder, wherein the rotational speed of ball-mill of ball mill is 300r/min, and the time of the ball milling is 8h;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into the pure titanium shell of hollow cylindrical structure, shell is vacuumized, shell to be evacuated is intracorporal Seal casinghousing after air;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1600 DEG C, pressure is 180MPa's Under the conditions of HIP sintering 1.5h, remove shell after natural cooling, obtain Ta-W-Al-Al2O3Alloy sintered compact;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1450 DEG C, extrusion ratio is 7 under conditions of into Row squeezes, and carries out the processing that strips off the skin after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3Alloy bar material, room temperature tensile intensity are 865MPa, room temperature elongation percentage It is 25%, 1700 DEG C of tensile strength is 410MPa, and material loss is 0.39mg/ after 100h is aoxidized in 1500 DEG C of air environments cm2, the Ta-W-Al-Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and anti- Oxidation susceptibility can use in 1500 DEG C of air environments.
A kind of embodiment 7: Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 10%, Al 4%, Al2O32.5%, surplus Ta, wherein described W, Al, Al2O3, Ta be powder raw material, the granularity of W powder and Al powder is equal No more than 30 μm, Al2O3The granularity of powder is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;The W powder, Al powder and Al2O3The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
The Ta-W-Al-Al2O3The preparation step of alloy bar material are as follows:
(1) tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, the ball milling under argon atmosphere protection It is uniformly mixed, obtains mixed-powder, wherein the rotational speed of ball-mill of ball mill is 300r/min, and the time of the ball milling is 8h;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into the pure titanium shell of hollow cylindrical structure, shell is vacuumized, shell to be evacuated is intracorporal Seal casinghousing after air;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1600 DEG C, pressure is 180MPa's Under the conditions of HIP sintering 1.5h, remove shell after natural cooling, obtain Ta-W-Al-Al2O3Alloy sintered compact;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1550 DEG C, extrusion ratio is 9 under conditions of into Row squeezes, and carries out the processing that strips off the skin after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3Alloy bar material, room temperature tensile intensity are 590MPa, room temperature elongation percentage It is 21%, 1700 DEG C of tensile strength is 388MPa, and material loss is 0.39mg/ after 100h is aoxidized in 1500 DEG C of air environments cm2, the Ta-W-Al-Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and anti- Oxidation susceptibility can use in 1500 DEG C of air environments.
A kind of embodiment 8: Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 12%, Al 5%, Al2O32%, surplus Ta, wherein described W, Al, Al2O3, Ta be powder raw material, the granularity of W powder and Al powder is not Greater than 30 μm, Al2O3The granularity of powder is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;W powder, Al powder and the Al2O3 The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
The Ta-W-Al-Al2O3The preparation step of alloy bar material are as follows:
(1) tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, the ball milling under argon atmosphere protection It is uniformly mixed, obtains mixed-powder, wherein the rotational speed of ball-mill of ball mill is 300r/min, and the time of the ball milling is 8h;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into the pure titanium shell of hollow cylindrical structure, shell is vacuumized, shell to be evacuated is intracorporal Seal casinghousing after air;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1600 DEG C, pressure is 180MPa's Under the conditions of HIP sintering 1.5h, remove shell after natural cooling, obtain Ta-W-Al-Al2O3Alloy sintered compact;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1550 DEG C, extrusion ratio is 9 under conditions of into Row squeezes, and carries out the processing that strips off the skin after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3Alloy bar material, room temperature tensile intensity are 620MPa, room temperature elongation percentage It is 23%, 1700 DEG C of tensile strength is 410MPa, and material loss is 0.55mg/ after 100h is aoxidized in 1500 DEG C of air environments cm2, the Ta-W-Al-Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and anti- Oxidation susceptibility can use in 1500 DEG C of air environments.
A kind of embodiment 9: Ta-W-Al-Al2O3Alloy bar material is made of the raw material of following mass percent: W 8%, Al 3%, Al2O33%, surplus Ta, wherein described W, Al, Al2O3, Ta be powder raw material, the granularity of W powder and Al powder is not Greater than 30 μm, Al2O3The granularity of powder is not more than 10 μm, and the granularity of Ta powder is not more than 50 μm;W powder, Al powder and the Al2O3 The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
The Ta-W-Al-Al2O3The preparation step of alloy bar material are as follows:
(1) tantalum powder, tungsten powder, aluminium powder and aluminum oxide powder are placed in ball mill, the ball milling under argon atmosphere protection It is uniformly mixed, obtains mixed-powder, wherein the rotational speed of ball-mill of ball mill is 300r/min, and the time of the ball milling is 8h;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into the pure titanium shell of hollow cylindrical structure, shell is vacuumized, shell to be evacuated is intracorporal Seal casinghousing after air;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1700 DEG C, pressure is 200MPa's Under the conditions of HIP sintering 1.5h, remove shell after natural cooling, obtain Ta-W-Al-Al2O3Alloy sintered compact;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1550 DEG C, extrusion ratio is 9 under conditions of into Row squeezes, and carries out the processing that strips off the skin after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
Ta-W-Al-Al manufactured in the present embodiment2O3Alloy bar material, room temperature tensile intensity are 828MPa, room temperature elongation percentage It is 25%, 1700 DEG C of tensile strength is 415MPa, and material loss is 0.33mg/ after 100h is aoxidized in 1500 DEG C of air environments cm2, the Ta-W-Al-Al2O3Alloy bar material has good temperature-room type plasticity and tensile strength, excellent Testing Tensile Strength at Elevated Temperature and anti- Oxidation susceptibility can use in 1500 DEG C of air environments.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (9)

1. a kind of Ta-W-Al-Al2O3Alloy bar material, which is characterized in that be made of the raw material of following mass percent: W 5%- 15%, Al 2%-6%, Al2O31%-4%, surplus Ta.
2. a kind of Ta-W-Al-Al according to claim 12O3Alloy bar material, which is characterized in that described W, Al, the Al2O3、 Ta is powder raw material, and wherein the granularity of W powder and Al powder is no more than 30 μm, Al2O3The granularity of powder is not more than 10 μm, Ta powder Granularity be not more than 50 μm.
3. a kind of Ta-W-Al-Al according to claim 22O3Alloy bar material, which is characterized in that the W powder, Al powder and Al2O3The quality purity of powder is not less than the quality purity of 99.9%, Ta powder not less than 99.5%.
4. a kind of Ta-W-Al-Al according to claim 12O3Alloy bar material, which is characterized in that by following mass percent Raw material be made: W 8%-12%, Al 3%-5%, Al2O32%-3%, surplus Ta.
5. a kind of Ta-W-Al-Al according to claim 42O3Alloy bar material, which is characterized in that by following mass percent Raw material be made: W 10%, Al 4%, Al2O32.5%, surplus Ta.
6. a kind of Ta-W-Al-Al2O3The preparation method of alloy bar material, which is characterized in that its preparation step are as follows: (1) by W, Al, Al2O3It is placed in ball mill with Ta, ball milling mixing is uniform under argon atmosphere protection, obtains mixed-powder;
(2) by the mixed-powder compression moulding, blank is obtained;
(3) blank is packed into shell, shell is vacuumized, seal casinghousing after the intracorporal air of shell to be evacuated;
(4) the intracorporal blank of shell will be sealed in be placed in hot isostatic pressing furnace, temperature is 1500 DEG C -1700 DEG C, pressure is HIP sintering 1h-3h under conditions of 160MPa-200MPa removes shell after natural cooling, obtains Ta-W-Al-Al2O3It closes Golden sintered body;
(5) by the Ta-W-Al-Al2O3Alloy sintered compact squeeze temperature be 1400 DEG C -1600 DEG C, the item that extrusion ratio is 6-10 It is squeezed under part, the processing that strips off the skin is carried out after natural cooling, obtains Ta-W-Al-Al2O3Alloy bar material.
7. a kind of Ta-W-Al-Al according to claim 62O3The preparation method of alloy bar material, which is characterized in that described The rotational speed of ball-mill of ball mill is 200r/min-400r/min in step (1), and the time of ball milling is 6h-12h.
8. a kind of Ta-W-Al-Al according to claim 62O3The preparation method of alloy bar material, which is characterized in that described Shell is hollow cylindrical structure in step (3), and the material of shell is pure titanium.
9. a kind of Ta-W-Al-Al according to claim 62O3The preparation method of alloy bar material, which is characterized in that described Ta-W-Al-Al in step (5)2O3The extruding temperature preferred scope of alloy sintered compact is 1450 DEG C -1550 DEG C, extrusion ratio 7-9.
CN201811168573.XA 2018-10-08 2018-10-08 A kind of Ta-W-Al-Al2O3Alloy bar material and preparation method Pending CN109234560A (en)

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CN109913726A (en) * 2019-05-06 2019-06-21 北方民族大学 A kind of Ta-W based alloy and preparation method thereof
CN112281039A (en) * 2020-11-13 2021-01-29 西安鑫昌机电设备有限责任公司 Ta-Hf-Zr-ZrB2Alloy bar and preparation method thereof

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CN109913726A (en) * 2019-05-06 2019-06-21 北方民族大学 A kind of Ta-W based alloy and preparation method thereof
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